#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003788.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003788 loop_ _publ_author_name 'Hook, J. M.' 'Dean, P. A. W.' 'Hockless, D. C. R.' _publ_section_title ; Hexakis(dimethyl sulfoxide)mercury(II) Trifluoromethanesulfonate, a Standard for Solid-State ^199^Hg NMR ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1547 _journal_page_last 1549 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C12 H36 Hg O6 S6,2(C F3 S O3)' _chemical_formula_sum 'C14 H36 F6 Hg O12 S8' _chemical_formula_weight 967.49 _space_group_IT_number 147 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3' _symmetry_space_group_name_H-M 'P -3' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 12.1950(10) _cell_length_b 12.1952 _cell_length_c 6.713(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 50.0 _cell_measurement_theta_min 48.8 _cell_volume 864.6(3) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection 'MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1989)' _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1993) ; _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Rigaku AFC6R' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator 'equatorial graphite' _diffrn_radiation_source 'Rigaku RU200B rotating Cu anode' _diffrn_radiation_type CuKalpha _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 8.12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1498 _diffrn_reflns_theta_max 60.12 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% -10.79 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 12.76 _exptl_absorpt_correction_T_max 0.354 _exptl_absorpt_correction_T_min 0.157 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_meas 0.000 _exptl_crystal_description block _exptl_crystal_F_000 478.00 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.04 _refine_diff_density_min -1.20 _refine_ls_extinction_coef 2E-6(2) _refine_ls_extinction_method 'Zachariasen (1968) type 2 Gaussian isotropic' _refine_ls_goodness_of_fit_obs 2.69 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 859 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0360 _refine_ls_shift/esd_max 0.0030 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ; w=4F~o~^2^/[\s^2^(F~o~^2^)+(0.009F~o~^2^)^2^] ; _refine_ls_wR_factor_obs 0.0460 _reflns_number_observed 859 _reflns_number_total 869 _reflns_observed_criterion >3\s(I) _[local]_cod_data_source_file hr1049.cif _[local]_cod_data_source_block James _cod_original_cell_volume 864.6(2) _cod_database_code 2003788 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -y, +x-y, +z' ' -x+y, -x, +z' ' -x, -y, -z' ' +y, -x+y, -z' ' +x-y, +x, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg(1) 0.0338(4) 0.0338 0.0452(5) 0.0169 0.0000 0.0000 S(1) 0.0430(10) 0.0410(10) 0.0420(10) 0.0206(9) -0.0045(8) -0.0011(8) S(2) 0.0460(10) 0.0461 0.059(2) 0.0231 0.0000 0.0000 F(1) 0.141(6) 0.091(5) 0.079(4) 0.070(5) -0.012(4) -0.027(3) O(1) 0.051(3) 0.046(3) 0.054(3) 0.025(3) -0.012(3) -0.006(3) O(2) 0.063(4) 0.061(4) 0.083(5) 0.011(3) 0.006(3) 0.016(3) C(1) 0.074(6) 0.057(5) 0.048(5) 0.037(5) -0.017(4) -0.008(4) C(2) 0.069(6) 0.087(7) 0.065(6) 0.051(6) 0.016(5) 0.014(5) C(3) 0.058(6) 0.0583 0.070(10) 0.0291 0.0000 0.0000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Hg(1) 0.0 0.0 0.0 0.0376(3) Uani S(1) 0.2141(2) -0.0540(2) 0.2176(3) 0.0420(10) Uani S(2) 0.6667 0.3333 -0.3568(5) 0.0510(10) Uani F(1) 0.6628(7) 0.2316(6) -0.7020(9) 0.098(4) Uani O(1) 0.1832(5) 0.0528(5) 0.1848(7) 0.050(3) Uani O(2) 0.5516(6) 0.2214(6) -0.3095(9) 0.078(4) Uani C(1) 0.2999(9) -0.0130(8) 0.4430(10) 0.059(5) Uani C(2) 0.3391(9) -0.0235(10) 0.0530(10) 0.069(5) Uani C(3) 0.6667 0.3333 -0.626(2) 0.061(6) Uani H(1a) 0.3221 -0.0753 0.4756 0.0702 Uiso H(1b) 0.3747 0.0670 0.4292 0.0702 Uiso H(1c) 0.2491 -0.0085 0.5470 0.0702 Uiso H(2a) 0.3612 -0.0876 0.0679 0.0821 Uiso H(2b) 0.3130 -0.0232 -0.0799 0.0821 Uiso H(2c) 0.4105 0.0566 0.0836 0.0821 Uiso loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.018 0.009 'International Tables' H 0.000 0.000 'International Tables' F 0.073 0.053 'International Tables' Hg -4.292 7.685 'International Tables' O 0.049 0.032 'International Tables' S 0.333 0.557 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 0 1 3 0 1 1 3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O(1) Hg(1) O(1) 2 94.6(2) yes O(1) S(1) C(1) ? 104.1(3) yes O(1) S(1) C(2) ? 106.5(4) yes C(1) S(1) C(2) ? 98.6(5) yes O(2) S(2) O(2) ? 115.1(2) ? O(2) S(2) C(3) ? 102.9(3) ? Hg(1) O(1) S(1) ? 116.4(3) yes S(2) C(3) F(1) ? 112.8(7) ? F(1) C(3) F(1) ? 105.9(8) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg(1) O(1) ? 2.347(5) yes S(1) O(1) ? 1.543(5) yes S(1) C(1) ? 1.766(8) yes S(1) C(2) ? 1.764(9) yes S(2) O(2) ? 1.421(6) ? S(2) C(3) ? 1.80(2) ? F(1) C(3) ? 1.321(8) ? Hg(1) H(1a) ? 5.48 yes Hg(1) H(1b) ? 5.11 yes Hg(1) H(1c) ? 4.80 yes Hg(1) H(2a) ? 5.05 yes Hg(1) H(2b) ? 4.00 yes Hg(1) H(2c) ? 4.73 yes Hg(1) H(1c) 1_554 4.73 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion Hg(1) O(1) S(1) C(1) -152.6(4) Hg(1) O(1) S(1) C(2) 103.8(4) S(1) O(1) Hg(1) O(1) 144.5(2) F(1) C(3) S(2) O(2) -59.5(4)